高等学校化学学报 ›› 2017, Vol. 38 ›› Issue (6): 1033.doi: 10.7503/cjcu20170068

• 分析化学 • 上一篇    下一篇

十八烷基离子液体杂化固相微萃取整体柱用于检测咖啡中的多环芳烃

张娜1, 万昕1, 宋旭燕2, 黄龙2, 郑京京3, 邢钧1()   

  1. 1. 生物医学分析化学教育部重点实验室, 武汉大学化学与分子科学学院, 武汉 430072
    2. 湖北中烟技术中心, 武汉 430051
    3. 武汉理工大学化学工程学院, 武汉 430079
  • 收稿日期:2017-02-03 出版日期:2017-06-10 发布日期:2017-05-23
  • 作者简介:联系人简介: 邢 钧, 男, 博士, 副教授, 主要从事色谱分析研究. E-mail: gc-ms@263.net
  • 基金资助:
    国家自然科学基金(批准号: 20775056)资助.

Application of Octadecyl Ionic Liquid Hybrid Solid-phase Microextraction Monolithic Column in the Detection of Polycyclic Aromatic Hydrocarbons in Coffee

ZHANG Na1, WAN Xin1, SONG Xuyan2, HUANG Long2, ZHENG Jingjing3, XING Jun1,*()   

  1. 1. Key Laboratory of Analytical Chemistry for Biology and Medicine(Ministry of Education), College of Chemistry and olecular Sciences, Wuhan University, Wuhan 430072, China
    2. Technology Center of Hubei Branch of China Tobacco Industry Corporation, Wuhan 430051, China
    3. School of Chemical Engineering, Wuhan University of Technology, Wuhan 430079, China
  • Received:2017-02-03 Online:2017-06-10 Published:2017-05-23
  • Contact: XING Jun E-mail:gc-ms@263.net
  • Supported by:
    † Supported by the National Natural Science Foundation of China(No.20775056).

摘要:

以自制的1-十八烷基-3-(γ-三乙氧基硅基丙基)咪唑溴盐离子液体(C18IL)、 二苯基二甲氧基硅烷(DDS)和四乙氧基硅烷(TEOS)为功能单体, 采用溶胶-凝胶法制备了烷基咪唑基离子液体管内固相微萃取整体柱(C18IL in-tube SPME). 以多环芳烃为分析对象, 考察了C18IL含量对C18IL in-tube SPME萃取性能的影响, 并对萃取条件进行了优化. 建立了基于C18IL in-tube SPME-气相色谱(GC-FID)的分析方法, 用于检测萘、 芴、 菲、 荧蒽和芘5种多环芳烃. 该方法的检出限(S/N=3)为0.007~0.072 μg/L, 定量限(S/N=10)为0.023~0.24 μg/L, 日内和日间精密度(RSD)除菲类多环芳烃外均小于10%. 将该方法用于检测咖啡中5种多环芳烃, 3个不同浓度下的加标回收率为85.79%~103.42%.

关键词: 离子液体, 整体柱, 管内固相微萃取, 多环芳烃

Abstract:

Ionic liquid of 1-octadecyl-3-(γ-triethoxysiliconpropyl)imidazole bromide(C18IL) was synthesized and then used as a functional monomer to produce the in-tube solid microextraction monolithic column(C18IL in-tube SPME) via sol-gel reaction. After that, five polycyclic aromatic hydrocarbons(PAHs), naphthalene, fluorine, phenanthrene, fluoranthene and pyrene, were employed as probe analytes to evaluate the preparation method of the column and optimize the extraction conditions. Finally, a method of C18IL in-tube SPME hyphen gas chromatography was established for the determination of PAHs in water. The limits of detection(LODs, S/N=3) were between 0.007 and 0.072 μg/L, and the limits of quantification(LOQs, S/N=10) varied from 0.023 to 0.24 μg/L. The intra- and inter-day relative standard deviations(RSDs) of the PAHs were below 10% except for that of phenanthrene. The proposed method was also applied to the determination of the PAHs in a coffee sample, and the recoveries for the five PHAs(spiked in the coffee sample at three levels) ranged from 85.79% to 103.42%.

Key words: Ionic liquid, Monolithic column, In-tube solid phase microextraction, Polycyclic aromatic hydrocarbons

中图分类号: 

TrendMD: